5468-22-4|3-Iodo-4,5-dimethoxybenzoic acid| Ambeed

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CAS No. :	5468-22-4
Formula :	C₉H₉IO₄
M.W :	308.07
SMILES Code :	O=C(O)C1=CC(OC)=C(OC)C(I)=C1

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H319
Precautionary Statements:	P264-P280-P305+P351+P338-P337+P313

Yield	Reaction Conditions	Operation in experiment
95%	With sodium chlorite; sodium dihydrogenphosphate; 2-methyl-but-2-ene; In water; tert-butyl alcohol; at 20℃; for 4h;Inert atmosphere;	3-Iodo-4,5-dimethoxybenzaldehyde (913 mg, 3.12 mmol) and 2-methyl-2-butene (3.10 mL) were dissolved in tert-butanol (10.0 mL), and a solution of 80% sodium chlorite (564 mg, 6.24 mmol) and monobasic sodium phosphate (487 mg 4.06 mmol) in water (7.00 mL) was added dropwise. The mixture was stirred for 4 h at room temperature. The solvent was removed in vacuo and the residue was diluted with water (40.0 mL). The pH of the solution was adjusted to 10 with 1 M aqueous NaOH, the aqueous phase was extracted with ether (2×20.0 mL). The aqueous layers were acidified to pH 2 by dropwise addition of 3 M aqueous HCl and extracted with ethyl acetate (3×25.0 mL). The combined organic layers were dried over anhydrous MgSO4 and the solvent was removed in vacuo to give a white solid. (Yield: 915 mg, 2.97 mmol, 95%). 1H NMR (d6-DMSO, 400 MHz, 20C): δ = 13.14 (br. s., 1H, COOH), 7.88 (d, J = 2.0 Hz, 1H,ArH), 7.53 (d, J = 1.8 Hz, 1H, ArH), 3.86 (s, 3H, OCH3), 3.77 (s, 3H, OCH3). 13C NMR (d6-DMSO, 100 MHz, 20C): δ = 166.5, 152.9, 152.8, 132.1, 129.3, 114.6, 93.2, 60.9, 56.9. ESMS calcd for C9H8IO4 [M-H]- : 306.9743, found 306.9750
	With sodium chlorite; aminosulfonic acid; In water; acetonitrile; at 20℃; for 0.833333h;	To a stirred solution of <strong>[32024-15-0]3-iodo-4,5-dimethoxybenzaldehyde</strong> (25.0 g, 85.6 mmol) in CH3CN [(800 ML)] at room temperature, was added a solution of sulfamic acid (10.65 g, 109 mmol) in [H20] (135 mL). To this was added, dropwise, a solution of NaClO2 (12.65 g, 112 mmol) in H20 (135 mL) over 20 min period. After stirring for a [FURTHER 30] min at room temperature, the solvent was removed in vacuo. The reaction was diluted [WITLI I.] HCl (700 mL) and extracted with EtOAc (3 x 300 mL). The combined organic layers were washed with brine (600 mL), dried over [NA2S04] and concentrated in vacuo to give 3,4- dimethoxy-5-iodobenzoic acid (26 [G).] The product was used without further purification.

Precautionary Statements-General
Code	Phrase
P101	If medical advice is needed,have product container or label at hand.
P102	Keep out of reach of children.
P103	Read label before use
Prevention
Code	Phrase
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P220	Keep/Store away from clothing/combustible materials.
P221	Take any precaution to avoid mixing with combustibles
P222	Do not allow contact with air.
P223	Keep away from any possible contact with water, because of violent reaction and possible flash fire.
P230	Keep wetted
P231	Handle under inert gas.
P232	Protect from moisture.
P233	Keep container tightly closed.
P234	Keep only in original container.
P235	Keep cool
P240	Ground/bond container and receiving equipment.
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P242	Use only non-sparking tools.
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P263	Avoid contact during pregnancy/while nursing.
P264	Wash hands thoroughly after handling.
P265	Wash skin thouroughly after handling.
P270	Do not eat, drink or smoke when using this product.
P271	Use only outdoors or in a well-ventilated area.
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P284	Wear respiratory protection.
P285	In case of inadequate ventilation wear respiratory protection.
P231 + P232	Handle under inert gas. Protect from moisture.
P235 + P410	Keep cool. Protect from sunlight.
Response
Code	Phrase
P301	IF SWALLOWED:
P304	IF INHALED:
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P320
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P321
P322
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P342	If experiencing respiratory symptoms:
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P378
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P391	Collect spillage. Hazardous to the aquatic environment
P301 + P310	IF SWALLOWED: Immediately call a POISON CENTER or doctor/physician.
P301 + P312	IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell.
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P302 + P334	IF ON SKIN: Immerse in cool water/wrap in wet bandages.
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P304 + P312	IF INHALED: Call a POISON CENTER or doctor/physician if you feel unwell.
P304 + P340	IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
P304 + P341	IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P305 + P351 + P338	IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing.
P306 + P360	IF ON CLOTHING: Rinse Immediately contaminated CLOTHING and SKIN with plenty of water before removing clothes.
P307 + P311	IF exposed: call a POISON CENTER or doctor/physician.
P308 + P313	IF exposed or concerned: Get medical advice/attention.
P309 + P311	IF exposed or if you feel unwell: call a POISON CENTER or doctor/physician.
P332 + P313	IF SKIN irritation occurs: Get medical advice/attention.
P333 + P313	IF SKIN irritation or rash occurs: Get medical advice/attention.
P335 + P334	Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
P337 + P313	IF eye irritation persists: Get medical advice/attention.
P342 + P311	IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician.
P370 + P376	In case of fire: Stop leak if safe to Do so.
P370 + P378	In case of fire:
P370 + P380	In case of fire: Evacuate area.
P370 + P380 + P375	In case of fire: Evacuate area. Fight fire remotely due to the risk of explosion.
P371 + P380 + P375	In case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion.
Storage
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P401
P402	Store in a dry place.
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P422
P402 + P404	Store in a dry place. Store in a closed container.
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P410 + P412	Protect from sunlight. Do not expose to temperatures exceeding 50 oC/122oF.
P411 + P235	Keep cool.
Disposal
Code	Phrase
P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

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CAS No.: 5468-22-4

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CAS No.: 5468-22-4

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Physical hazards
Code	Phrase
H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
H203	Explosive; fire, blast or projection hazard
H204	Fire or projection hazard
H205	May mass explode in fire
H220	Extremely flammable gas
H221	Flammable gas
H222	Extremely flammable aerosol
H223	Flammable aerosol
H224	Extremely flammable liquid and vapour
H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
H227	Combustible liquid
H228	Flammable solid
H229	Pressurized container: may burst if heated
H230	May react explosively even in the absence of air
H231	May react explosively even in the absence of air at elevated pressure and/or temperature
H240	Heating may cause an explosion
H241	Heating may cause a fire or explosion
H242	Heating may cause a fire
H250	Catches fire spontaneously if exposed to air
H251	Self-heating; may catch fire
H252	Self-heating in large quantities; may catch fire
H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
H270	May cause or intensify fire; oxidizer
H271	May cause fire or explosion; strong oxidizer
H272	May intensify fire; oxidizer
H280	Contains gas under pressure; may explode if heated
H281	Contains refrigerated gas; may cause cryogenic burns or injury
H290	May be corrosive to metals
Health hazards
Code	Phrase
H300	Fatal if swallowed
H301	Toxic if swallowed
H302	Harmful if swallowed
H303	May be harmful if swallowed